関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 反応物 | 2,2-Difluoroethan-1-ol | HCID 136187 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,2-Difluoroethyl trifluoromethanesulfonate | HCID 2774089 | 75% |
反応手順
In a flask under argon was placed triflic anhydride (10.22 mL, 61 mmol) and dichloromethane (10 mL) and it was cooled to −70° C. To this cooled mixture was added slowly a solution of 2,2-difluoroethanol (5.00 g, 61 mmol) and triethylamine (8.5 mL, 61 mmol) in dichloromethane (10 mL). After the addition was complete, the mixture was warmed to 25° C. and then concentrated in vacuo. This material was distilled at 60° C. and 50 mm Hg which afforded trifluoro-methanesulfonic acid 2,2-difluoro-ethyl ester (9.74 g, 75%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741327B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-7ce4d0728fee45208e0af46ba190a52b |
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| 出典メモ | uspto-grants-2010_06 |
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